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Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
25 July 2016 to 26 August 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
European Community (EC), EC no. 440/2008, Part A: Methods for the Determination of Physico-Chemical Properties, Guideline A.1: “Melting/Freezing Temperature”, Official Journal of the European Union no. L142, May 31, 2008.
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
Organization for Economic Co-operation and Development (OECD), OECD Guidelines for the Testing of Chemicals no. 102: "Melting Point / Melting Range", July 27, 1995.
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
United States Environmental Protection Agency (EPA), Product Properties Test Guidelines no. OPPTS 830.7200: "Melting Point/Melting Range", March 1998.
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
No further details specified
Key result
Melting / freezing pt.:
162 °C
Atm. press.:
1 013.25 hPa
Decomposition:
no
Sublimation:
no

Preliminary test

At approximately 70°C a mechanical shock was observed. This did not influence the measurement. From 200°C upwards the weight of the sample decreased significantly. At 272°C the sample weight had decreased by 25%.

After the experiment no test item was observed in the sample container.

 

Main study

One minor and one major endothermic peak between 125°C and 175°C were observed. The extrapolated onset temperature of the minor peak was 149.39°C. This signal was most probably linked to the presence of an impurity or another crystallographic species. The extrapolated onset temperature of the major peak was 162.17°C. Both effects were most likely obtained due to melting.

To investigate the melting peaks between 125°C and 175°C a repeated heating cycle was applied in the Experiment 2. A closed sample container was applied to investigate the endothermic peak between 250°C and 325°C.

With the first heating the extrapolated onset temperature of the melting peak was 149.39°C. The extrapolated onset temperature of the second peak was 162.29°C.

During cooling no effects were observed which were due to crystallization of the test item (results are archived in the raw data).

During the second heating a glass transition was observed between 25°C and 50°C. The inflection point of the glass transition was 40.53°C. An exothermic peak was observed between 50°C and 125°C. The effect was obtained due to cold crystallization of the test item.

The extrapolated onset temperature of the first (minor) melting peak was 159.82°C. The peak maximum of the second (major) melting peak was 163.85°C. The extrapolated onset and the peak maximum were not used for calculating the melting temperature, since it was obtained by melting of non-original test item.

The melting temperature was determined as the average melting temperature obtained from experiment 1 (162.17°C) and experiment 2 (162.29°C).

Conclusions:
The melting temperature of Lowinox® 22IB46 was determined at 162°C (435K) using DSC.
Executive summary:

The purpose of the study was to determine the physico-chemical properties for Lowinox® 22IB46.

 

The melting temperature of the test item were determined using differential scanning calorimetry (DSC), in accordance with the following guidelines:

European Community (EC), EC no. 440/2008, Part A: Methods for the Determination of Physico-Chemical Properties, Guideline A.1: “Melting/Freezing Temperature”, Official Journal of the European Union no. L142, May 31, 2008.

Organization for Economic Co-operation and Development (OECD), OECD Guidelines for the Testing of Chemicals no. 102: "Melting Point / Melting Range", July 27, 1995.

United States Environmental Protection Agency (EPA), Product Properties Test Guidelines no. OPPTS 830.7200: "Melting Point/Melting Range", March 1998.

 

The melting temperature of Lowinox® 22IB46 was determined at 162°C (435K) using DSC.

Description of key information

Key value determined in a GLP accredited laboratory study using DSC in accordance with EU Method A.1, OECD Guideline 102 and US EPA Procedure OPPT 830.7200.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
162 °C

Additional information